US5221484A - Catalytic filtration device and method - Google Patents
Catalytic filtration device and method Download PDFInfo
- Publication number
- US5221484A US5221484A US07/811,307 US81130791A US5221484A US 5221484 A US5221484 A US 5221484A US 81130791 A US81130791 A US 81130791A US 5221484 A US5221484 A US 5221484A
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- US
- United States
- Prior art keywords
- face
- catalyst
- particulate
- feed stock
- filtrate
- Prior art date
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- Expired - Lifetime
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 52
- 238000001914 filtration Methods 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000003054 catalyst Substances 0.000 claims abstract description 121
- 239000012528 membrane Substances 0.000 claims abstract description 70
- 239000011148 porous material Substances 0.000 claims abstract description 60
- 239000000706 filtrate Substances 0.000 claims abstract description 38
- 239000012065 filter cake Substances 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000010574 gas phase reaction Methods 0.000 claims abstract description 8
- 239000012982 microporous membrane Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims description 57
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 27
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- 239000000919 ceramic Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 13
- 239000007789 gas Substances 0.000 claims description 11
- 239000012018 catalyst precursor Substances 0.000 claims description 9
- 238000006555 catalytic reaction Methods 0.000 claims description 9
- 238000005470 impregnation Methods 0.000 claims description 9
- 238000011010 flushing procedure Methods 0.000 claims description 8
- 230000003647 oxidation Effects 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 8
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- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 description 3
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Images
Classifications
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- B01D39/2068—Other inorganic materials, e.g. ceramics
- B01D39/2072—Other inorganic materials, e.g. ceramics the material being particulate or granular
- B01D39/2075—Other inorganic materials, e.g. ceramics the material being particulate or granular sintered or bonded by inorganic agents
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- B01D46/66—Regeneration of the filtering material or filter elements inside the filter
- B01D46/70—Regeneration of the filtering material or filter elements inside the filter by acting counter-currently on the filtering surface, e.g. by flushing on the non-cake side of the filter
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- B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
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- B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
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- B01D46/2425—Honeycomb filters characterized by parameters related to the physical properties of the honeycomb structure material
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- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
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- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8631—Processes characterised by a specific device
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/022—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous
- F01N3/0222—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters characterised by specially adapted filtering structure, e.g. honeycomb, mesh or fibrous the structure being monolithic, e.g. honeycombs
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/023—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles
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- F01N3/02—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust
- F01N3/021—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters
- F01N3/023—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles
- F01N3/0233—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for cooling, or for removing solid constituents of, exhaust by means of filters using means for regenerating the filters, e.g. by burning trapped particles periodically cleaning filter by blowing a gas through the filter in a direction opposite to exhaust flow, e.g. exposing filter to engine air intake
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/24—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by constructional aspects of converting apparatus
- F01N3/28—Construction of catalytic reactors
- F01N3/2882—Catalytic reactors combined or associated with other devices, e.g. exhaust silencers or other exhaust purification devices
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- B01D2275/30—Porosity of filtering material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D2321/04—Backflushing
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- B01D2321/20—By influencing the flow
- B01D2321/2033—By influencing the flow dynamically
- B01D2321/2058—By influencing the flow dynamically by vibration of the membrane, e.g. with an actuator
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- B01D2321/30—Mechanical cleaning, e.g. with brushes or scrapers
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- B01D46/24—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies
- B01D46/2403—Particle separators, e.g. dust precipitators, using rigid hollow filter bodies characterised by the physical shape or structure of the filtering element
- B01D46/2418—Honeycomb filters
- B01D46/2451—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure
- B01D46/2455—Honeycomb filters characterized by the geometrical structure, shape, pattern or configuration or parameters related to the geometry of the structure of the whole honeycomb or segments
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- F01N2250/00—Combinations of different methods of purification
- F01N2250/02—Combinations of different methods of purification filtering and catalytic conversion
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL COMBUSTION ENGINES
- F01N2330/00—Structure of catalyst support or particle filter
- F01N2330/06—Ceramic, e.g. monoliths
Definitions
- the invention disclosed in U.S. Ser. No. 07/639,568 relates to a particulate filter, regenerable by back-flushing, formed from a porous honeycomb monolith structure with selectively plugged passageways and a microporous membrane coating applied to the passageway surfaces.
- This continuation-in-part application further includes a catalyst coating within or on the filter, which becomes a catalytic filter, capable of reacting constituents in the filtrate fluid as it passes through the filter.
- heterogeneous catalysts and catalyst devices which are used to carry out a great number of chemical reactions.
- the reaction rate for a catalyst device can be limited by the rate of bulk mass transfer of reactants to the catalyst surface or by the rate of pore diffusion of reactants within the pore structure of porous heterogeneous catalysts.
- Such limitations are widely described in the technical literature, for example in the books "The Role Of Diffusion In Catalysis", by C. N. Satterfield and T. K. Sherwood, published by Addison-Wesley Publishing Company (1963) and "Heterogeneous Catalysis In Practice", by C. N. Satterfield, published by McGraw-Hill Book Company (1980).
- the engineering design of heterogeneous catalytic reactors is frequently based on these limitations. New catalyst configurations which can reduce or perhaps even eliminate such mass transfer limitations would have substantial practical value.
- This device consists of fiberglass fabrics which are coated with vanadium oxide catalysts, which in the presence of added ammonia, efficiently remove particulates as a filter and reduce the oxides of nitrogen in the gas flowing through the fabric filter. This latter process is called selective catalytic reduction (SCR).
- SCR selective catalytic reduction
- catalyst coated filters One advantage of such catalyst coated filters is that two processes can be achieved in a single device. In the above instance, the processes are particulate removal and catalytic reduction of a gaseous contaminant.
- a further advantage of such a catalytic filtration process is that particulate matter can be removed before the filtered fluid contacts the catalyst. In cases in which particulate matter poisons the catalyst, this prefiltration can prolong catalyst life. This can be important, for example, in SCR systems for reduction of oxides of nitrogen in combustion streams containing ash catalyst poisons.
- a catalytic filter in contrast to flowing over or around a catalyst coated support.
- a reactant fluid flows through a packed bed of catalyst particles, and both bulk and pore diffusion limitations, as indicated above, can limit the reaction rate.
- other catalytic reactor devices such as monolith supported catalysts in which the reactant fluid flows through the passageways of a monolith support onto which a catalyst coating has been applied.
- the reactant fluid flows through the pore structure of the catalyst, which is in fact the catalyst-coated filter. This flow configuration can greatly reduce or even eliminate bulk diffusion or pore diffusion limitations present in other more traditional catalytic reactors.
- the catalytic filter disclosed herein has the advantages of substantially eliminating diffusional limitations present in many heterogeneously catalyzed reactions, a very high compactness for a catalytic filter, and a capability for high temperature service.
- the device of this invention has wide utility for filtration of gases and liquids while concurrently catalyzing a reaction within the filtered fluid.
- Applications of special importance are found in the field of air pollution control for combustion gases from which fly ash can be removed while simultaneously removing gaseous contaminants such as oxides of nitrogen, sulfur dioxide, and volatile organic vapors.
- Other applications for air pollution control and coal gasification exist in which it is desirable to remove particulate matter, followed by catalyzing a reaction of one or more gaseous species present.
- oxidation processes to remove organic vapors from a variety of industrial sources may be used to remove a variety of air toxics enumerated in the 1990 Amendments to the Clean Air Act of 1970.
- the amendment identifies 189 air toxics, mainly organics, emitted by a variety of sources which must be controlled.
- a still further object is to provide a catalyst reactor in which mass transfer limitations associated with bulk gas mass transfer and pore diffusion are substantially reduced.
- This invention features a catalytic filtration device for separating a particulate-containing feed stock into a filtrate and a particulate-containing filter cake.
- the device is comprised of a monolith of porous material containing a plurality of passageways extending longitudinally from an inlet end face to an outlet end face, having a plurality of plugs in the ends of the passageways at the inlet end face and at the outlet end face to prevent direct passage of the feed stock through the passageways from the inlet end face to the outlet end face.
- a microporous membrane selected to separate the feed stock into a filtrate and particulate-containing filter cake is applied to at least the wall surfaces of the passageways open at the inlet end face and the membrane has a mean pore size smaller than the mean pore size of the porous material.
- the device is regenerable by withdrawal of the filter cake from the inlet end face of the device.
- a catalyst is applied to the device for catalyzing a reaction in the filtrate as it passes through the device.
- the catalytic filtration device has the catalyst applied to the interstitial pore volume of the device.
- the catalyst in the interstitial pore volume of the device may be applied by impregnation of the filter with a solution of a catalyst precursor.
- the catalyst may be applied as a discrete layer of a high surface area particulate catalyst carrier support which is itself coated with the catalyst.
- the high surface area particulate catalyst carrier support may be applied to the downstream side of the monolith passageway walls.
- the high surface area particulate catalyst carrier support may be applied between the membrane coating and the monolith passageway walls.
- the catalytic filtration device has a filtration surface area per unit volume greater than about thirty square feet per cubic foot.
- the mean pore diameter of the membrane coating is from about 0.1 micron to 5 microns.
- the catalytic filtration device may be regenerated by back-flushing with a fluid.
- the catalytic filtration device is suitable for catalyzing a gas phase reaction.
- One gas phase reaction which may be catalyzed is the reduction of oxides of nitrogen.
- Another gas phase reaction which may be catalyzed is the oxidation of sulfur dioxide.
- Yet another gas phase reaction which may be catalyzed is the oxidation of volatile organic vapors.
- the monolith porous material is ceramic and the membrane coating applied thereto is also ceramic.
- This invention also features a method for the preparation of a catalytic filtration device for separating a particulate-containing feed stock into a filtrate and a particulate-containing filter cake, comprising: providing a monolith of porous material containing a plurality of passageways extending longitudinally from an inlet end face to an outlet end face, having a plurality of plugs in the ends of the passageways at the inlet end face and at the outlet end face to prevent direct passage of the feed stock through the passageways from the inlet end face to the outlet end face; applying a microporous membrane selected to separate the feed stock into a filtrate and particulate-containing filter cake to at least the wall surfaces of the passageways open at the inlet end face and of mean pore size smaller than the mean pore size of the porous material; and applying a catalyst the device for catalyzing a reaction in the filtrate as it passes through the device.
- the method for the preparation of a catalytic filtration device may include applying the catalyst within the interstitial pore volume of the device. This method may further include impregnating the filter with a solution of a catalyst precursor to form the catalyst.
- the method for the preparation of a catalytic filtration device may include applying the catalyst as a discrete layer of a high surface area particulate catalyst carrier support which is itself coated with the catalyst.
- the high surface area particulate catalyst carrier support may be applied to the outlet side of the monolith passageway walls, or it may be applied between the membrane coating and the monolith passageway walls.
- the invention also includes the catalytic filtration device prepared by any of the above methods.
- the invention further includes a method for the filtration and catalytic reaction of a particulate-containing fluid feed stock, comprising: introducing a fluid feed stock into the inlet end passageways of the catalytic filtration device; filtering the fluid feed stock by the catalytic filter to provide a filtrate and a particulate-containing filter cake; catalyzing a reaction in the filtrate as the filtrate passes through the device; and regenerating the device by withdrawal of the filter cake from the inlet end face of the device.
- This method for the filtration and catalytic reaction of a particulate-containing fluid feed may include introducing a gaseous feed stock as the fluid feed stock and catalyzing a reaction in the gaseous filtrate.
- the gas phase reaction may include the reduction of the oxides of nitrogen, the oxidation of sulfur dioxide, or the oxidation of organic vapors.
- All of the above methods may further include back flushing the device periodically with a fluid to remove the filter cake.
- FIG. 1 shows a enlarged sectional view of a membrane-coated monolith filter structure along a plane parallel to an axis of the structure and perpendicular to the planes of the monolith end faces.
- FIG. 2 shows an enlarged sectional view of a membrane-coated passageway wall of the filter with catalyst particles dispersed within and throughout the filter passageway wall and membrane coating.
- FIG. 3 shows an enlarged sectional view of a membrane coated passageway wall of the filter further coated on the downstream side with a catalyst coating comprised of a high surface area particulate catalyst carrier, itself coated with catalyst.
- FIG. 4 shows an enlarged sectional view of a membrane coated passageway wall of the filter with a catalyst coating comprised of a high surface area particulate catalyst carrier, itself coated with catalyst, applied between the membrane and the passageway wall.
- the invention includes a porous monolith 10 in a housing 12 which contains a plurality of longitudinal passageways extending from an inlet end face 16 to an outlet end face 18 of the monolith.
- a filter body is formed from such a monolith by plugging alternate ends of adjacent passageways, with plugs 20 and 24, thereby creating inlet and outlet passageways 22 and 26 of the filter. This construction prevents direct passage of a feed stock through the passageways from the inlet end face to the outlet end face of the monolith through which filtrate is discharged.
- a thin microporous membrane 28 is formed on the surfaces of the passageway walls 14 on at least the inlet passageways.
- the pore size of the membrane is smaller than that of the monolith material, and preferably less than that of the size of the particulate matter to be removed by the filter.
- the catalyst can be applied within the membrane-coated filter, i.e., in its interstitial pore volume. This can be achieved, for example, by impregnation of the filter with a solution of a catalyst precursor, followed by drying, calcining, and other possible treatments of a catalyst precursor material.
- the catalyst could also be applied within the interstitial pore volume by other techniques, such as chemical vapor deposition or plasma deposition.
- FIG. 2 shows an enlarged sectional view of a membrane-coated passageway wall which contains catalyst particles deposited within the interstitial pore volume.
- the monolith passageway wall 30 supports a membrane coating 32.
- Catalyst particles 34 are dispersed throughout the membrane-coated filter. Fluid being filtered 36 flows through the membrane coating and underlying passageway wall. After suspended particles are removed by the membrane coating, the filtered fluid or filtrate is brought into direct contact with the catalyst particles as the filtrate flows through the interstitial pore volume.
- the filter can be impregnated with a solution of ammonium metavanadate. After drying and calcining, the vanadium oxide catalyst will be distributed through the pores of the monolith filter support and its membrane coating.
- Other additives to the impregnation solution such as a titanium, tungsten, and molybdenum salts, can be added as catalyst stabilizers or promoters.
- the precursor can be a solution of a salt, such as chloroplatinic acid, which after drying, calcining, and reducing with hydrogen yields a dispersed platinum metal catalyst.
- a salt such as chloroplatinic acid
- a palladium chloride solution can be used for impregnation.
- Analogous metallic salts can be used to impregnate the filter with precursors for other metal catalysts, or mixtures thereof After calcination, the deposited oxides can be reduced to yield the dispersed metal catalyst.
- the catalyst can be applied as a discrete layer of a high surface area particulate catalyst carrier support which itself is impregnated with the catalyst precursor or catalyst.
- FIG. 3 shows such a layer 40 applied to the downstream side of the monolith passageway wall 42. Fluid feed flow 44 flows through the membrane coating 46, in this example applied to both sides of the passageway wall, through the passageway wall 42, and the catalyst coating layer 40.
- the particulate carrier coating can be applied by the same methods which can be used to apply a membrane coating.
- the particulate carrier coating is normally stabilized by a thermal treatment to bond the carrier particles.
- the active catalyst can be applied to the particulate carrier, by methods described above for direct application to a membrane-coated filter, either before or after the carrier is applied to the filter. If the active catalyst is applied after the particulate carrier is bonded to the filter, the active catalyst particles can be dispersed throughout the device.
- the advantages of using a second carrier coating for the catalyst relate to surface area of the active catalyst.
- Both the porous monolith support and, normally, the membrane coating will have a relatively low surface area.
- the resulting surface area of the active catalyst may be low.
- the catalyst coating consists of a high surface area particulate carrier support onto which the active catalyst is applied, the resulting surface area of the active catalyst material can be larger than that achieved by impregnation of a low surface area membrane-coated filter.
- the principal function of the membrane coating is to have a uniform and controlled pore size so as to effectively retain particles in the fluid to be filtered. It is less limiting in choice of membrane forming materials to have the separate catalyst coating which can be prepared without concern about interstitial pore size distribution.
- the catalyst can be applied as a catalyst-impregnated carrier coating located between the membrane coating and the passageway wall of the monolith filter support on the inlet passageway side, as shown in FIG. 4.
- the separate catalyst layer 50 is deposited before applying the membrane coating 52 to the monolith passageway wall 54.
- Feed fluid 56 is thereby constrained to flow first through the membrane coating, then the discrete catalyst carrier layer, and finally through the passageway wall.
- the catalyst carrier coating with overlying membrane coating can be applied to either the feed side or the filtrate side of the passageway wall.
- Such separate catalyst carrier coatings and membrane coatings can be applied in various combinations to either or both of the inlet and outlet monolith passageways in one or more layers.
- the catalyst carrier coating can be applied either beneath or on top of the membrane coating on either or both sides of the monolith passageway walls. If the separate catalyst carrier coating is applied directly to a porous monolith, some of the carrier material may penetrate into the pore structure of the monolith porous material. In this instance, the applied catalyst coated thereon together with the carrier may lie within the monolith pore structure.
- the porous monolith can be formed from a variety of porous materials, including ceramics, glass-bonded ceramics, glasses, sintered metals, cermets, resins or organic polymers, papers or textile fabrics, and various combinations thereof.
- ceramics include cordierite, alumina, silica, mullite, zirconia, titania, spinel, silicon carbide, silicon nitride, and mixtures thereof. These ceramic materials may also be used in monoliths in which the ceramic materials are bonded with a glass.
- the mean pore diameter of the monolith material should be greater than about 5 microns, and the porosity of the material should be greater than about 40 volume percent.
- the plugs used to seal the alternate ends of the adjacent passageways can be polymeric or inorganic, and are normally selected to have good adhesion and chemical and thermal compatibility with the monolith material.
- the membrane coating can be formed from a Variety of materials, including polymeric membranes and inorganic membranes.
- Inorganic materials which can be used include sintered metals and ceramic membranes.
- Ceramic membranes can include alumina, zirconia, titania, silica, zircon, cordierite, mullite, spinel, silicon carbide, silicon nitride, and mixtures thereof, bonded by thermal sintering or with a reactive inorganic binder.
- Mean pore diameter of the membrane coating is preferably in the range of from about 0.1 micron to 5 microns.
- the thickness of the membrane coating should be as thin as possible so as to minimize the hydraulic resistance of the membrane coating, preferably less than 100 microns.
- the membrane coating may be applied only to the inlet passageways, or alternately, it may be applied to both inlet and outlet passageways. If applied to both sets of passageways, the clean filter resistance to flow is increased. However, a membrane coating on the outlet passageways prevents possible plugging of the monolith material by particulate matter which may be present in a back-flushing fluid.
- the membrane coating may be applied by several techniques, such as by viscous coating, filtration, and slip casting. Viscous coating is useful for coating of polymeric membranes. Filtration and slip casting may be used to apply coatings of ceramic or metal powders, which are subsequently stabilized and made strongly coherent and adherent to the passageway walls by thermal sintering, chemical reaction bonding, or other bonding techniques.
- the catalyst can be applied to a membrane coated monolith filter support by impregnation with a solution containing a soluble catalyst precursor. After drying and calcining to decompose the precursor material, and possibly including a chemical reduction step, the catalyst will be dispersed throughout the monolith support and its membrane coating.
- the pore structure be largely free of defects, such as cracks, or large pores which can allow particulate matter to pass through the filter.
- a coating of a catalyst impregnated particulate carrier can have defects and large pores as it does not serve as a particulate removal barrier. Any such pores or defects, however, should not lead to unacceptable channeling of process fluid, which will not occur if the major resistance to filtrate flow is other than in the catalyst coating.
- Catalysts can be metals or metal mixtures, including the noble metals platinum, palladium, rhodium, ruthenium, and mixtures thereof, or other metals such as copper, nickel, and silver.
- the catalyst can be comprised of an oxide or oxide mixtures, including oxides of aluminum, cerium, chromium, cobalt, copper, iron, magnesium, manganese, molybdenum, nickel, potassium, titanium, tungsten, vanadium, zinc, as well as alumina silicate zeolites.
- the high surface area particulate carrier support can be a porous alumina, silica, activated carbon, titania, or other porous catalyst support material.
- the porous support layer can be applied by the techniques used to coat inorganic membranes, as disclosed in U.S. Pat. No. 4,983,423, which is incorporated by reference herein.
- the filter may be used to filter either a gaseous or liquid feed stock.
- gas phase applications in which the membrane coated, catalyst filter can find use. These include, for example, the filtration of combustion flue gas in which fly ash is removed by filtration and gaseous contaminants are reacted as they pass through the filter. Such contaminants can include oxides of nitrogen which can be reduced to nitrogen and water vapor, sulfur dioxide which can be oxidized to sulfur trioxide, and unburned organic vapors which can be oxidized to carbon dioxide and water vapor.
- filtration applications in coal gasification processes where it is desirable to remove particulate ash and to react contaminants in the process gas stream.
- an exhaust gas contains both fine particulate matter and organic vapor contaminants which can be removed simultaneously by filtration and oxidation.
- the filter may be regenerated, i.e. particulate matter removed, by back-flushing with a fluid normally free of particulate matter.
- the fluid used for back-flushing can be filtrate produced from the feed stock.
- the filter can be regenerated by mounting in an upflow orientation and removing the particulate matter by vibration, rapping, or other mechanical means.
- the substrate for the catalyst coating was a ceramic membrane-coated monolith.
- the monolith was a cylinder 1" in diameter and 2" long.
- the monolith contained a multiplicity of parallel passageways extending from one end to the opposite end.
- the passageway configuration was square with 100 cells per square inch.
- the passageway dimension was 0.083" and the passageway wall thickness was 0.017".
- the monolith material was EX47 cordierite (Corning, Inc.) with a mean pore size of 12 microns and a porosity of 50%.
- the monolith was coated in accordance with the methods taught in U.S. Pat. No. 4,983,423 with the ceramic membrane described in U.S. patent application Ser. No. 07/639,568.
- the membrane-coated monolith was saturated with a solution of catalyst precursor.
- This solution contained 150 milliliters of water filtered with a 50,000 molecular weight cut-off ultrafiltration membrane and 10.5 grams of ammonium Vanadate (Aldrich Chemical Co., 99% NH 4 VO 3 ). This is slightly above the solubility limit at 96° C. (6.95 grams per 100 milliliters of water) so as to ensure a saturated solution.
- the solution was formed by heating the stirred components for approximately 2 hours to about 96° C.
- the hot saturated solution was held without stirring to allow undissolved salt to settle, and the coated monolith, which had been heated to 90-95° C., was immersed in the hot supernatant vanadate solution for 6.5 minutes.
- the saturated monolith was then withdrawn from the solution and immediately immersed in a glass beaker containing 250 milliliters of 3° C. isopropanol (2-Propanol, Aldrich Chemical Co., 99%+, A.C.S. Reagent Grade) which was cooled in an ice water bath. Quenching was used to precipitate the vanadate within the monolith structure due to the decreased solubility at low temperature (0.52 grams per 100 milliliters of water at 15° C.). Isopropanol was used because it is miscible with water but not a solvent for ammonium metavanadate. As a result, a solvent exchange between the alcohol and water takes place within the monolith while keeping the vanadate in the precipitated form.
- the monolith to be dried easily at room temperature. If thermal drying of the coated monolith were attempted with water in the pore volume, the vanadate could redissolve and migrate with the drying front as water was removed from the monolith. During quenching, a small amount of yellowish precipitate formed in the isopropanol. The coated monolith remained in the alcohol for about one minute during which the temperature rose only slightly.
- the coated monolith was then removed, placed on a paper towel, and allowed to dry for several minutes. Little vanadate was extracted by the paper towel. The monolith had a slight yellowish color.
- the sample was heated in air to 400° C. at a rate of about 2° C. per minute in a resistively heated kiln. After reaching temperature, the kiln was turned off and allowed to cool overnight. After firing, the monolith had turned a uniform dark reddish orange color indicative of vanadium pentoxide. Weight uptake due to the fired impregnant was about 18 milligrams of vanadia per gram of membrane-coated monolith. This corresponds to a catalyst volume of about 1 to 2 percent of the monolith pore volume.
- the monolith passageways were then plugged with a low temperature setting cement (Adhesive No. 919, Cotronics Corp.) so as to form a dead-ended filter which was then tested for gas flow/ pressure drop characteristics.
- a low temperature setting cement Adhesive No. 919, Cotronics Corp.
- the plugging and pressure drop measurement were performed according to the procedures taught in U.S. patent application Ser. No. 07/639,568.
- the internal filter surface area after plugging was about 0.06 square feet.
- the measured pressure drop of the filter was about 5 inches of water column at 10 cubic feet per hour nitrogen gas flow which corresponds to about 2.8 feet per minute face velocity. This pressure drop was not measurably different from the pressure drop for a membrane coated filter sample without the catalyst applied.
- the catalyst impregnated filter was used in a test as a device for selective catalytic reduction of oxides of nitrogen.
- the catalytic filter sample was installed in a test apparatus in which a mixture of 600 ppm NO in air was passed through the sample at 380° C., with NH 3 addition at a molar ratio of NH 3 to NO of 1:1, and a gas flow rate of 1 std liter/minute. This corresponds to a space velocity (SV) at standard temperature and pressure (STP) of about 2300 hr -1 or filter face velocity of about 1.3 ft/min.
- SV space velocity
- STP standard temperature and pressure
- the removal of NO by selective catalytic reduction was measured to be about 70%. However, it was determined subsequently that a portion of the NH 3 was removed by background reactions in the test system. Accordingly, the degree of removal of NO may have been limited by the amount of NH 3 reactant present, not by other limitations.
- This membrane-coated filter was further coated by a catalyst manufacturer with a discrete layer of a high surface area particulate catalyst carrier support which itself was impregnated with a proprietary NO x reduction catalyst. This layer was applied to the outlet passageway wall surfaces on top of the membrane coating.
- the catalytic filter so prepared was tested for NO reduction. Test conditions were 400 ppm NO in air at 400° C., an NH 3 slip (unreacted NH 3 in product gas) of 10 ppm, and a space velocity of 14,000 hr -1 at STP. Greater than 85% NO removal was measured.
Abstract
Description
Claims (28)
Priority Applications (9)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US07/811,307 US5221484A (en) | 1991-01-10 | 1991-12-20 | Catalytic filtration device and method |
AT93901925T ATE170420T1 (en) | 1991-12-20 | 1992-12-18 | CATALYTIC FILTRATION SYSTEM AND METHOD |
ES93901925T ES2121987T3 (en) | 1991-12-20 | 1992-12-18 | CATALYTIC FILTRATION DEVICE AND METHOD. |
EP93901925A EP0619757B1 (en) | 1991-12-20 | 1992-12-18 | Catalytic filtration device and method |
DK93901925T DK0619757T3 (en) | 1991-12-20 | 1992-12-18 | Catalytic filtration device and method |
PCT/US1992/011106 WO1993012867A1 (en) | 1991-12-20 | 1992-12-18 | Catalytic filtration device and method |
JP51183793A JP3261382B2 (en) | 1991-12-20 | 1992-12-18 | Catalytic filtration device and method |
AU33326/93A AU3332693A (en) | 1991-12-20 | 1992-12-18 | Catalytic filtration device and method |
DE69226873T DE69226873T2 (en) | 1991-12-20 | 1992-12-18 | CATALYTIC FILTRATION PLANT AND METHOD |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US07/639,568 US5114581A (en) | 1991-01-10 | 1991-01-10 | Back-flushable filtration device and method of forming and using same |
US07/811,307 US5221484A (en) | 1991-01-10 | 1991-12-20 | Catalytic filtration device and method |
Related Parent Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US07/639,568 Continuation-In-Part US5114581A (en) | 1991-01-10 | 1991-01-10 | Back-flushable filtration device and method of forming and using same |
Publications (1)
Publication Number | Publication Date |
---|---|
US5221484A true US5221484A (en) | 1993-06-22 |
Family
ID=25206181
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US07/811,307 Expired - Lifetime US5221484A (en) | 1991-01-10 | 1991-12-20 | Catalytic filtration device and method |
Country Status (9)
Country | Link |
---|---|
US (1) | US5221484A (en) |
EP (1) | EP0619757B1 (en) |
JP (1) | JP3261382B2 (en) |
AT (1) | ATE170420T1 (en) |
AU (1) | AU3332693A (en) |
DE (1) | DE69226873T2 (en) |
DK (1) | DK0619757T3 (en) |
ES (1) | ES2121987T3 (en) |
WO (1) | WO1993012867A1 (en) |
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DE69226873T2 (en) | 1999-01-21 |
AU3332693A (en) | 1993-07-28 |
DE69226873D1 (en) | 1998-10-08 |
JP3261382B2 (en) | 2002-02-25 |
WO1993012867A1 (en) | 1993-07-08 |
EP0619757A1 (en) | 1994-10-19 |
EP0619757B1 (en) | 1998-09-02 |
ATE170420T1 (en) | 1998-09-15 |
JPH07505083A (en) | 1995-06-08 |
ES2121987T3 (en) | 1998-12-16 |
DK0619757T3 (en) | 1999-05-31 |
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